2,4-Dichlorophenol → (2,4-Dichlorophenoxy)propanol

HRID 1939150노트

반응식

HRID 1939150 반응식
Br[CH2:2][CH2:3][CH2:4][OH:5].[Cl:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[OH:14].N12CCCN=C1CCCCC2>C(O)(C)C.C(Cl)Cl>[Cl:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[O:14][CH2:2][CH2:3][CH2:4][OH:5]

참가 물질

6

반응물 3

HCID 84492,4-DichlorophenolHCID 123083-Bromo-1-propanolHCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene

생성물 1

HCID 235019(2,4-Dichlorophenoxy)propanol수율 105.9%

시약·촉매·용매 2

HCID 3776Isopropanol용매2회HCID 6344Dichloromethane용매

실험 절차

A solution of 3-bromopropanol (53.86 g, 0.368 mol) in isopropanol is added dropwise to a mixture of 2,4-dichlorophenol (50 g, 0.307 mol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (70.05 g, 0.406 mol) in isopropanol at reflux. The reaction mixture is heated at reflux for 3 hours and concentrated in vacuo to obtain a residue. The residue is dissolved in methylene chloride and the organic solution is washed sequentially with 0.5N sodium hydroxide solution, 1M hydrochloric acid and brine, dried over MgSO4 and concentrated in vacuo to obtain an oil which solidifies to give the title product as a white solid (71.9 g, mp 53°-55° C.).

후처리

  1. temperatureat reflux
  2. temperatureThe reaction mixture is heated
  3. temperatureat reflux for 3 hours
  4. concentrationconcentrated in vacuo
  5. customto obtain a residue
  6. washthe organic solution is washed sequentially with 0.5N sodium hydroxide solution, 1M hydrochloric acid and brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo
  9. customto obtain an oil which

출처 및 근거

ORD 기록
ord-de05edcca3cf4b73852ddb71d1874a57
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05696050

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